U.S. patent number 3,969,337 [Application Number 05/455,484] was granted by the patent office on 1976-07-13 for chromatographic fractionation of whey.
This patent grant is currently assigned to Boehringer Mannheim G.m.b.H.. Invention is credited to Friedrich Batz, Karl Lauer, Georg Stoeck.
United States Patent |
3,969,337 |
Lauer , et al. |
July 13, 1976 |
Chromatographic fractionation of whey
Abstract
The process for the chromatographic fractionation of whey
comprising passing whey through a column of an ion exchange
material, thereafter passing water through said column as eluant,
and collecting the aqueous effluent from said column as a plurality
of fractions. Advantageously the ion exchange material is a
polystyrene resin containing sulfonic acid groups neutralized with
calcium ions and cross-linked with about 2 to 4% by weight of
divinyl-benzene, and the eluant is demineralized water.
Inventors: |
Lauer; Karl (Schriesheim,
DT), Stoeck; Georg (Mannheim-Waldhof, DT),
Batz; Friedrich (Lampertheim, DT) |
Assignee: |
Boehringer Mannheim G.m.b.H.
(Mannheim, DT)
|
Family
ID: |
5878464 |
Appl.
No.: |
05/455,484 |
Filed: |
March 27, 1974 |
Foreign Application Priority Data
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|
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Apr 18, 1973 [DT] |
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2319581 |
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Current U.S.
Class: |
530/416; 210/656;
530/366; 530/833; 530/365; 530/386 |
Current CPC
Class: |
A23C
9/1465 (20130101); A23C 9/148 (20130101); A23J
1/205 (20130101); B01J 39/26 (20130101); G01N
33/04 (20130101); A23V 2002/00 (20130101); A23V
2002/00 (20130101); A23V 2300/30 (20130101); Y10S
530/833 (20130101) |
Current International
Class: |
A23C
9/146 (20060101); A23C 9/00 (20060101); A23C
9/148 (20060101); A23J 1/20 (20060101); A23J
1/00 (20060101); B01J 39/26 (20060101); G01N
33/02 (20060101); G01N 33/04 (20060101); A23J
001/20 () |
Field of
Search: |
;260/112R,121,122 |
References Cited
[Referenced By]
U.S. Patent Documents
Other References
Biochimica et Biophysica Acta, 100(1965) 154-162, Groves
Dissertation Abstracts, Morrison, vol. 23, 1962. .
Chem. Abstracts, vol. 64, 1966, 10171c- 10171e, Szuchet et al.
.
Chem. Abstracts, vol. 54, 1960, 23102i- 23103c, Schober et al.
.
Biochimica et Biophysica Acta, 214(1970) 419-426, Armstrong et al.
.
Advances in Protein Chemistry, 1967, p. 142, McKenzie. .
Lab Manual of Analytical Methods of Protein Chem. vol. I, pp.
67-78, Alexander..
|
Primary Examiner: Schain; Howard E.
Attorney, Agent or Firm: Burgess, Dinklage & Sprung
Claims
What is claimed is:
1. The process for the chromatographic fractionation of dairy whey
containing lactose, proteins and mineral salts into a protein
fraction comprising passing said whey through a column of a cation
exchange material in neutral form, said cation exchange material
comprising a polystyrene resin containing sulfonic acid groups,
thereafter passing an aqueous eluant consisting essentially of
water through said column, and collecting a plurality of sequential
aqueous effluents from said column as a plurality of separate
fractions.
2. The process according to claim 1, wherein the ion exchange
material is a polystyrene resin containing sulfonic acid
groups.
3. The process according to claim 1, wherein the cation exchange
material is neutralized with calcium ions.
4. The process according to claim 1, wherein the ion exchange
material used has a low degree of cross-linking.
5. The process according to claim 1, wherein the ion exchange
material used has a divinyl-benzene content of about 2 to 4% by
weight.
6. The process according to claim 1, wherein the eluant is
demineralized water.
7. The process according to claim 1, wherein the whey is
concentrated before passage through the column.
8. The process according to claim 7, wherein the ion exchange
material is a polystyrene resin containing sulfonic acid groups
neutralized with calcium ions and cross-linked with about 2 to 4%
by weight of divinyl-benzene, and the eluant is demineralized
water.
Description
The present invention is concerned with a process for the
chromatographic fractionation of whey.
The solids content of liquid whey is about 7%, of which about 5% is
lactose, 0.9% is proteins and 0.5 - 1% is mineral salts. Sour whey
contains somewhat less lactose but, in place thereof, more lactic
acid.
As is known from numerous publications, whey protein is of
extraordinary importance for human nutrition and experimental
plants for the separation of lactalbumin and lactoglobulin have
already been set up throughout the world. Generally, it is
important to avoid a heat treatment of the whey in order to be able
to obtain the protein in a native state. For the separation of the
proteins, there have previously been used reversible osmosis,
electrodialysis and fractionation with the use of a molecular
sieve, for example "Sephadex". This latter process is the subject
matter of U.S. Patent Specification No. 3,547,900. Without doubt,
column chromatography with the use of a molecular sieve is
indicated for such a separation because molecular sieves are able
to distinguish very easily between large and small molecules.
Surprisingly, we have now found that the separation of whey or of a
whey concentrate into the components protein (lactalbumin or
lactoglobulin), lactose and salts, such as calcium lactate, takes
place even more effectively on a suitable ion exchanger.
Thus, according to the present invention, there is provided a
process for the chromatographic separation of whey, wherein whey is
chromatographed on an ion exchanger, using water as the eluant.
Examples of ion exchangers which can be used for the process
according to the present invention include polystyrene resins
containing sulfonic acid groups (cation exchangers). The ion
exchangers used have preferably been converted into neutral form by
means of suitable cations, preferably by calcium cations.
Ion exchangers, for example polystyrene resins, are especially
preferred which have a low degree of cross-linking, e.g. those
corresponding to a divinyl-benzene content of about 2-4% by weight
being especially preferred.
As eluant, it is especially preferred to use water which has been
demineralized, if necessary.
The effective separation of the solid components present in whey
with the help of the process according to the present invention is
surprising because ion exchangers, in contradistinction to
molecular sieves, cannot themselves distinguish between large and
small molecules. It is also surprising that no denaturing takes
place on the exchangers and thus an irreversible bonding of the
protein does not occur. As a result of these surprising
discoveries, there are obtained the following advantages for a
large-scale utilization of the new process according to the present
invention:
1. The contamination of sewage and waste water disposal systems by
dairies is an extraordinarily important problem for the protection
of the environment. It can be substantially avoided in an economic
manner by the use of a separation plant operating according to the
process of the present invention.
2. According to previously known methods, whey is first
concentrated in order to separate out crystalline lactose. This
step is now superfluous since the separation of lactose takes place
in one step on the ion exchanger.
3. The thermolabile protein is separated in a very gentle manner
and is obtained in the form of a pale, water-soluble product.
4. Inorganic salts and calcium lactate are also separated in an
excellent manner.
5. At a given flowthrough rate, the pressure drop along the ion
exchanger is considerably less than in the case of the use of a
column of a molecular sieve, so that it is possible to operate on a
large scale with higher throughput rates.
6. Since elution is carried out with water, the separation column
can, without further treatment, be used immediately for the next
cycle.
The following Example is given for the purpose of illustrating the
present invention:
Example
6 liters of sour whey having a solids contents of 7.2% by weight
are concentrated in a vacuum at 40.degree.C to a six-fold solids
concentration. This concentrate (about 1000ml) is applied at
20.degree.C to a separation column of 10 cm diameter and 4 m
length. The column is filled with a cation exchanger (polystyrene
resin containing sulfonic acid groups: Lewatite TSW-40), which is
quantitatively loaded with calcium ions. The resin, prior to
sulfonation, was produced by polymerizing styrene with 4% by weight
of divinyl-benzene as cross-linking agent.
10 Liters of demineralized water are run through the column at
20.degree.C and then fractions are collected with the next 22
liters of water. The composition of the fractions is given in the
following Table:
TABLE ______________________________________ eluate protein lactose
intermediate calcium (liters) (g) (g) runnings (g) lactate (g)
______________________________________ 10-13.5 48.4 -- -- --
13.5-19 -- 284 -- -- 19-26 -- -- 17 -- 26-32 -- -- -- 82
______________________________________
The protein fraction is gently evaporated in a vacuum at
40.degree.C. The resultant product, which is obtained in the form
of almost colorless flakes, is completely water-soluble.
The lactose (284 g) is, after concentration, obtained in
crystalline form.
The column is directly ready for another cycle of
fractionation.
The rate at which the whey or its concentrate percolates through
the column may be varied widely but preferably is such that the
residence time in the column is at least about 1 hour and
preferably at least about 4 hours.
It will be appreciated that the instant specification and examples
are set forth by way of illustration and not limitation, and that
various modifications and changes may be made without departing
from the spirit and scope of the present invention.
* * * * *